WO2021229840A1 - 透光性高靭化ジルコニア焼結体 - Google Patents

透光性高靭化ジルコニア焼結体 Download PDF

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Publication number
WO2021229840A1
WO2021229840A1 PCT/JP2020/039387 JP2020039387W WO2021229840A1 WO 2021229840 A1 WO2021229840 A1 WO 2021229840A1 JP 2020039387 W JP2020039387 W JP 2020039387W WO 2021229840 A1 WO2021229840 A1 WO 2021229840A1
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Prior art keywords
sintered body
zirconia sintered
sample
oxide
zirconia
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English (en)
French (fr)
Japanese (ja)
Inventor
清治 伴
勤 杉山
裕太 安岡
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Hitachi Construction Machinery Co Ltd
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KCM Corp
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Priority to JP2022522500A priority Critical patent/JP7367207B2/ja
Publication of WO2021229840A1 publication Critical patent/WO2021229840A1/ja
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    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61C—DENTISTRY; APPARATUS OR METHODS FOR ORAL OR DENTAL HYGIENE
    • A61C13/00—Dental prostheses; Making same
    • A61C13/08—Artificial teeth; Making same
    • A61C13/083—Porcelain or ceramic teeth
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61C—DENTISTRY; APPARATUS OR METHODS FOR ORAL OR DENTAL HYGIENE
    • A61C5/00—Filling or capping teeth
    • A61C5/70—Tooth crowns; Making thereof
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/48—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zirconium or hafnium oxides, zirconates, zircon or hafnates
    • C04B35/486—Fine ceramics
    • C04B35/488—Composites

Definitions

  • the present invention relates to a zirconia sintered body, and more particularly to a translucent and highly toughened zirconia sintered body that can be advantageously used as a dental restoration material.
  • zirconia sintered bodies (partially stabilized zirconia sintered bodies) in which a small amount of rare earth oxides such as yttrium oxide (Y 2 O 3) are solid-dissolved as a stabilizer have high strength and high toughness. Therefore, it is used in various industrial products such as structural materials in various machines such as cutting tools, bearings and crushers, and biological materials such as dental restoration materials.
  • rare earth oxides such as yttrium oxide (Y 2 O 3)
  • Y 2 O 3 yttrium oxide
  • the partially stabilized zirconia sintered body when used as a dental restoration material, the partially stabilized zirconia sintered body has not only mechanical properties such as high strength and high toughness, but also a color tone from an aesthetic point of view. Optical characteristics such as yttria-stabil and translucency are also required. As a method for increasing the translucency of the partially stabilized zirconia sintered body, it is conceivable to increase the content of a stabilizer such as yttria oxide.
  • the partially stabilized zirconia sintered body is only partially stabilized, there is a problem that long-term stability is particularly difficult in a hydrothermal environment.
  • a partially stabilized zirconia sintered body undergoes a phase transition from tetragonal to monoclinic when heated in the presence of moisture.
  • the strength of the sintered body decreases due to the growth of microcracks caused by the volume expansion of about 4% accompanying this phase transition. Therefore, in order to use the partially stabilized zirconia sintered body in an industrial product, it is necessary to use a sintered body in which the progress of the phase transition is sufficiently suppressed according to the application of the industrial product, the environment in which it is used, and the like.
  • Patent Document 1 Japanese Unexamined Patent Publication No. 2012-412319
  • the partially stabilized zirconia is contained as a matrix phase
  • the phosphorus (P) element and the boron (B) element are contained in the zirconia sintered body.
  • zirconia sintered bodies each of which is contained in a predetermined ratio with respect to the mass.
  • the progress of the phase transition is suppressed without deteriorating the mechanical properties of the sintered body by introducing the phosphorus (P) element and the boron (B) element.
  • the translucency required as a dental restoration material cannot be fully exhibited due to the increase in the interface due to the different phase such as the glass phase and the residual pores.
  • Patent Document 2 Japanese Unexamined Patent Publication No. 2015-143178
  • yttrium oxide exceeding 4.0 mol% and 6.5 mol% or less and alumina of less than 0.1 wt% are contained, and the relative density is 99.82. % Or more
  • the total light transmittance for light having a wavelength of 600 nm at a thickness of 1.0 mm is 37% or more and less than 40%
  • the bending strength is 500 MPa or more.
  • the translucent zirconia sintered body disclosed in the same document does not have sufficient mechanical properties, and for example, when used as a dental restoration material, it is used for anterior teeth. It can only be used for some products such as crown restorations, and when used, the sintered body used so that the product exhibits sufficient mechanical properties. It is necessary to make the thickness above a certain level.
  • Patent Document 3 Japanese Unexamined Patent Publication No. 2014-185078
  • it is composed of zirconia containing 2 to 4 mol% yttrium oxide and less than 0.1 wt% alumina as an additive, and has a relative density of 99.8% or more.
  • a translucent zirconia sintered body characterized by having a total light transmittance of 35% or more and a crystal grain size of 0.20 to 0.45 ⁇ m at a thickness of 1.0 mm.
  • the translucent zirconia sintered body disclosed in the same document was used as a crown restoration for molar teeth. Although it was a sintered body having sufficient translucency, it was found that it did not have sufficient translucency for use as a crown restoration for anterior teeth.
  • Patent Document 4 Japanese Unexamined Patent Publication No. 1-108162 is formed by mixing zirconia with at least 0.3 to 25% by weight of niobium and one or more niobium-based substances.
  • Zirconia ceramics sintered body characterized by the above are disclosed.
  • the sintered body disclosed in the same document exhibits high bending strength and excellent fracture toughness, since the niobium compound particles are present between the zirconia particles, the light generated by the niobium compound particles which are different components Due to the influence of refraction, scattering, etc., there is a risk that translucency will be insufficient for use as a constituent material for crown restorations.
  • sintered bodies that can be particularly suitably used as dental restoration materials, specifically, have high fracture toughness. It is desired to develop a zirconia sintered body having excellent translucency and also excellent water heat deterioration resistance.
  • the present invention has been made in the background of such circumstances, and the problem to be solved thereof is that it has excellent fracture toughness, exhibits excellent translucency, and exhibits excellent translucency. It is an object of the present invention to provide a zirconia sintered body having excellent water heat resistance deterioration characteristics.
  • the present invention contains yttrium oxide and / or ytterbium oxide as a stabilizer in a proportion of 3.5 to 5.0 mol%, and also contains niobium oxide and / or tantalum oxide at 0. It is composed of zirconia contained in a ratio of 3 to 1.5 mol%, has a fracture toughness value of 4.5 MPa ⁇ m or more, and has an capacity of 80.0% or less at a thickness of 1.5 mm. The gist of this is the zirconia sintered body.
  • the present invention also has a gist of a dental restoration material made of the zirconia sintered body of the above-described embodiment.
  • the zirconia sintered body according to the present invention has excellent mechanical properties that can be sufficiently used as a dental restoration material because 1) the fracture toughness value is 4.5 MPa ⁇ m or more. 2) Since the opacity at a thickness of 1.5 mm is 80.0% or less, it exhibits excellent translucency to the extent that it can be suitably used as a dental restoration material. Further, the zirconia sintered body of the present invention is excellent as described above because it contains yttrium oxide and / or ytterbium oxide and niobium oxide and / or tantalum oxide in a predetermined ratio, respectively. In addition to exhibiting mechanical properties and translucency, it also exhibits excellent water and heat resistance deterioration characteristics.
  • the zirconia sintered body according to the present invention having such excellent properties can be used particularly advantageously as a dental restoration material, and the thickness of the sintered body can be reduced. Not only can it be used as a constituent material for a crown restoration for molar teeth, but it can also be sufficiently used as a constituent material for a crown restoration for anterior teeth.
  • the zirconia sintered body according to the present invention contains yttrium oxide and / or ytterbium oxide [ytterbium oxide (III)] as a stabilizer as a first essential component in a proportion of 3.5 to 5.0 mol%, and the first
  • the second essential component is zirconia containing niobium oxide and / or tantalum oxide in a proportion of 0.3 to 1.5 mol%.
  • the zirconia sintered body may be simply referred to as a sintered body.
  • the content ratio of the first essential component is less than 3.5 mol%
  • fracture toughness is achieved even if niobium oxide and / or tantalum oxide is contained at the ratio of the present invention.
  • the value is excellent, there is a possibility that a sintered body exhibiting sufficient translucency (in other words, a sintered body having an capacity of 80.0% or less at a thickness of 1.5 mm) cannot be obtained. ..
  • the ratio exceeds 5.0 mol%, even if niobium oxide and / or tantalum oxide is contained at the ratio of the present invention, at least one of fracture toughness and translucency is not sufficient.
  • the content ratio of the total amount of the first essential component is within the range of 3.5 to 5.0 mol%. Needless to say, it is done.
  • the content ratio of the second essential component is less than 0.3 mol%, even if yttrium oxide and / or ytterbium oxide is contained at the ratio of the present invention, sintering is performed. The body may not be able to exert sufficient fracture toughness. On the other hand, if the ratio exceeds 1.5 mol%, the sintered body may not exhibit sufficient translucency even if niobium oxide and / or tantalum oxide is contained at the ratio of the present invention. be.
  • the content ratio of the total amount of the second essential component is 0.3 to 1.5 mol%, as in the case of the first essential component described above. It is considered to be within the range.
  • the zirconia sintered body having an capacity of 80.0% or less at 1.5 mm is the zirconia sintered body according to the present invention.
  • the fracture toughness value (unit: MPa ⁇ m) in the present specification and claims is the IF specified in JIS R 1607: 2015 "Room temperature fracture toughness test method for fine ceramics”. It is measured according to the law.
  • Opacity is also referred to as opacity among those skilled in the art of ceramics.
  • the outline of the opacity is shown in FIG. Where light is indicated by an arrow in FIG. 1, the opacity in the present specification and claims is 1) one in a zirconia sintered body having a thickness of 1.5 mm (hereinafter referred to as a sample in this paragraph).
  • Reflectance measured when a white body with a reflectance close to 100% is applied to the surface of the sample (backed state): R 0
  • R 0 Reflectance measured when a white body with a reflectance close to 100% is applied to the surface of the sample (backed state): R 0
  • R 0 Reflectance measured when a white body with a reflectance close to 100% is applied to the surface of the sample (backed state)
  • R 0 Reflectance measured when a white body with a reflectance close to 100% is applied to the surface of the sample (backed state)
  • R 0 a state in which a black body is applied to one surface of
  • the opacity is 100%, indicating that the sample is a completely opaque material, while if the reflectance: R 1 is 0, the opacity is 0. %, which indicates that the sample is completely transparent.
  • yttrium oxide and / or ytterbium oxide and niobium oxide and / or tantalum oxide are each contained in a predetermined ratio, so 1)
  • the fracture toughness value is 4.5 MPa ⁇ m or more and exhibits excellent mechanical properties, and 2) the capacity at a thickness of 1.5 mm is 80.0% or less, and also exhibits excellent translucency. In addition, 3) it also exhibits excellent water and heat resistance deterioration characteristics.
  • the zirconia sintered body of the present invention may contain components other than the above-mentioned two essential components within a quantitative range as long as the object of the present invention is not impaired.
  • the content ratio of alumina Al 2 O 3
  • alumina may precipitate between the zirconia particles and the translucency may be deteriorated. Therefore, the content ratio of alumina is 0.05% by mass. The following is preferable.
  • the zirconia sintered body according to the present invention described above can be advantageously produced, for example, according to the production method described in detail below.
  • a zirconia sintered body containing only yttrium oxide as the first essential component First, a zirconia powder containing yttrium oxide and a second essential component (niobium oxide and / or tantalum oxide) are prepared. 1) After mixing them with a mixer, 2) add a binder such as PVA, and 3) spray dry. 4) The dried mixture is molded to obtain a molded product, and 5) the obtained molded product is calcined by firing under normal pressure to obtain the desired yttrium oxide and niobium oxide and / or tantalum oxide. The contained zirconia sintered body can be obtained.
  • a zirconia sintered body containing yttrium oxide and / or ytterbium oxide as a first essential component zirconia sol, yttrium compound providing yttrium oxide during sintering body after sintering (e.g., YCl 3), ytterbium compound providing ytterbium oxide during sintering body after sintering (e.g., YbCl 3), as well as the Prepare the second essential component (niobium oxide and / or tantalum oxide).
  • the dried product is crushed in a milk pot or the like, 11) the obtained crushed product is molded to obtain a molded product, and 12) the obtained molded product is fired under normal pressure and sintered to obtain ytterbium oxide. And / or a zirconia sintered body containing ytterbium oxide and niobium oxide and / or tantalum oxide can be obtained.
  • niobium pentoxide as niobium oxide (Nb 2 O 5), but also tantalum pentoxide as tantalum oxide (Ta 2 O 5) is advantageously
  • the form of the oxide or the like when mixed with the first essential component is not particularly limited, and a powdery substance, a sol-like substance or the like can be appropriately used, and the particle size is advantageous. Small (fine) powders and sol-like substances with a small (average particle size) are used.
  • the zirconia sintered body according to the present invention is not limited to those produced by the above-mentioned first and second production methods, and can also be produced by combining various conventionally known methods. be.
  • the zirconia sintered body manufactured as described above has excellent fracture toughness, exhibits excellent translucency, and also has excellent water and heat deterioration resistance.
  • zirconia sintered bodies (Sample Nos. 1-44) were produced by appropriately using the following raw materials.
  • the firing of the molded body when producing the zirconia sintered body (sample) was carried out under the conditions of 1500 ° C. (heat retention time: 2 hours) under normal pressure for all the zirconia sintered bodies (sample).
  • Example No. 1 Manufacture of 1- A binder was added to the 2.0Y-ZrO 2 powder, spray-dried, and then the dried mixture was filled in a mold ( ⁇ 20 mm). After applying a pressure of 0.78 MPa to the mold, a disk-shaped molded product was taken out from the mold, and CIP molding was performed on the molded product at a pressure of 196 MPa. A zirconia sintered body (Sample No. 1) was produced by firing the molded body after CIP molding.
  • Example No. 2 Manufacture of 2- Except for using 3.0Y-ZrO 2 powder instead of 2.0Y-ZrO 2 powder Sample No. A molded product was produced according to the same method as in No. 1, and the zirconia sintered body (Sample No. 2) was produced by firing the molded product.
  • Example No. 4 Manufacturing of 4- Sample No. except that a predetermined amount of Ta 2 O 5 powder was used instead of the predetermined amount of Nb 2 O 5 powder.
  • a molded product was produced according to the same method as in No. 3, and a zirconia sintered body (Sample No. 4) was produced by firing the molded product.
  • the dried product was crushed in a mortar, and the obtained crushed product was filled in a mold ( ⁇ 20 mm). After applying a pressure of 0.78 MPa to the mold, a disk-shaped molded product was taken out from the mold, and CIP molding was performed on the molded product at a pressure of 196 MPa.
  • a zirconia sintered body (Sample No. 5) was produced by firing the molded body after CIP molding.
  • the dried product was crushed in a mortar, and the obtained crushed product was filled in a mold ( ⁇ 20 mm). After applying a pressure of 0.78 MPa to the mold, a disk-shaped molded product was taken out from the mold, and CIP molding was performed on the molded product at a pressure of 196 MPa.
  • a zirconia sintered body (Sample Nos. 6 to 10) was produced by firing the molded body after CIP molding.
  • Example No. 11 Manufacturing of 11- Except for using 4.2Y-ZrO 2 powder instead of 2.0Y-ZrO 2 powder Sample No. A molded product was produced according to the same method as in No. 1, and the zirconia sintered body (Sample No. 11) was produced by firing the molded product.
  • a molded product was produced according to the same method as in 12 to 18, and the zirconia sintered body (Sample Nos. 19 and 20) was produced by firing the molded product.
  • Example No. Manufacture of 21-23- Instead of Nb 2 O 5 powder of a predetermined amount, Nb 2 O 5 powder and Ta 2 O 5 powder was used instead of the prescribed amounts of sample No.
  • a molded product was produced according to the same method as in 12 to 18, and the zirconia sintered body (Sample Nos. 21 to 23) was produced by firing the molded product.
  • the dried product was crushed in a mortar, and the obtained crushed product was filled in a mold ( ⁇ 20 mm). After applying a pressure of 0.78 MPa to the mold, a disk-shaped molded product was taken out from the mold, and CIP molding was performed on the molded product at a pressure of 196 MPa.
  • a zirconia sintered body (Sample No. 24) was produced by firing the molded body after CIP molding.
  • the dried product was crushed in a mortar, and the obtained crushed product was filled in a mold ( ⁇ 20 mm). After applying a pressure of 0.78 MPa to the mold, a disk-shaped molded product was taken out from the mold, and CIP molding was performed on the molded product at a pressure of 196 MPa.
  • a zirconia sintered body (Sample Nos. 25 to 27) was produced by firing the molded body after CIP molding.
  • Example No. 28 Manufacture of 28- ZrO 2 sol, except for changing the amount of YCl 3 and YbCl 3
  • Sample No. A molded product was produced according to the same method as in No. 5, and a zirconia sintered body (Sample No. 28) was produced by firing the molded product.
  • Example No. 29 Manufacture of 29- ZrO 2 sol, except for changing each amount of YCl 3, YbCl 3 and Nb 2 O 5 powder sample No.
  • a molded product was produced according to the same method as in 6 to 10, and the zirconia sintered body (Sample No. 29) was produced by firing the molded product.
  • a molded product was produced according to the same method as in 6 to 10, and the zirconia sintered body (Sample Nos. 31 to 33) was produced by firing the molded product.
  • Example No. Manufacture of 37, 38- Sample No. except that a predetermined amount of Ta 2 O 5 powder was used instead of the predetermined amount of Nb 2 O 5 powder.
  • a molded product was produced according to the same method as in 34 to 36, and the zirconia sintered body (Sample Nos. 37, 38) was produced by firing the molded product.
  • Example No. 39 Manufacture of 39- Except for using 5.6Y-ZrO 2 powder instead of 2.0Y-ZrO 2 powder Sample No. A molded product was produced according to the same method as in No. 1, and the zirconia sintered body (Sample No. 39) was produced by firing the molded product.
  • Example No. Manufacture of 40, 41- Each predetermined amount of 5.6Y-ZrO 2 powder and Nb 2 O 5 powder was put into a pot mill (crushing ball: zirconia ball ⁇ 1 mm), and crushed and mixed in the pot mill for 1 hour. Then, a binder was added to the mixture, and the mixture was spray-dried, and then the dried mixture was filled in a mold ( ⁇ 20 mm). After applying a pressure of 0.78 MPa to the mold, a disk-shaped molded product was taken out from the mold, and CIP molding was performed on the molded product at a pressure of 196 MPa. A zirconia sintered body (Sample No. 40, 41) was produced by firing the molded body after CIP molding.
  • Example No. 42 Manufacture- Sample No. except that the amounts of ZrO 2 sol and YbCl 3 used were changed.
  • a molded product was produced according to the same method as in No. 5, and a zirconia sintered body (Sample No. 42) was produced by firing the molded product.
  • a molded product was produced according to the same method as in 6 to 10, and the zirconia sintered body (Sample Nos. 43, 44) was produced by firing the molded product.
  • the fracture toughness value was measured according to the method shown below, and the opacity at a thickness of 1.5 mm was determined.
  • a spectrophotometer (product name: CM-3700d) manufactured by Konica Minolta Co., Ltd., a disk-shaped test piece with a thickness of 1.5 mm cut out from each sample was tested with a white body backed.
  • the reflectance (R 0 ) of the body and the reflectance (R 1 ) of the test body with the black body backed were measured.
  • the spectrophotometer used is configured to automatically calculate the opacity from the measurement results, and when measuring the reflectance, a white calibration plate (product name: CM-A90, product name: CM-A90, as a white body) is used as a white body.
  • a zero calibration box (product name: CM-A94, standard accessory of CM-3700d) was used as a black body (standard accessory of CM-3700d).
  • “reflection” is used for the item “reflection / transmission”
  • “SCI method” is used for the item “specular reflected light processing”
  • “MAV (8 mm)” is used for the item “measurement diameter”. ) ”,“ 100% Full ”for the item“ UV condition ”,“ 10 ° ”for the item“ visual field ”, and“ D65 ”for the item“ main light source ”.
  • sample No. For each zirconia sintered body according to 11, 15 to 17, the monoclinic phase ratio (%) after hydrothermal treatment was measured according to the method shown below. Specifically, the surface of each sample (sintered body) is mirror-polished with diamond abrasive grains (particle size: 3 ⁇ m), and the polished sample is subjected to an autoclave (device name: SN200, Yamato Kagaku Co., Ltd.). Water heat deterioration treatment at 134 ° C (steam pressure: 0.22 MPa) x 5 hours, 134 ° C (steam pressure: 0.22 MPa) x 15 hours, 134 ° C (steam pressure: 0.22 MPa) x 30 hours.
  • the X-ray diffraction pattern of the polished surface of the sample after each treatment time has elapsed is measured with an X-ray diffractometer (device name: Ultima IV, manufactured by Rigaku Co., Ltd.). Then, using the measurement result, the monoclinic phase ratio (%) was obtained from the following formula. As can be understood from the following equation, the monoclinic phase ratio corresponds to the X-ray diffraction peak intensity [Im (111)] corresponding to the monoclinic phase (111) plane and the monoclinic phase (11-1) plane.
  • X-ray detector D / tex Ultra (accessory device) ⁇ Scan speed: 2.0 ° / min ⁇ Sampling width: 0.02 ° ⁇ Divergence slit: 1.0 mm ⁇ Divergent vertical slit: 10 mm ⁇ Scattering slit: 8 mm ⁇ Light receiving slit: open ⁇ Voltage: 40kV ⁇ Current: 40mA ⁇ Measurement area: 26-38 °
  • the zirconia sintered body according to the present invention As is clear from Tables 1 and 2, and the zirconia sintered body according to the present invention (Sample Nos. 6 to 10, 13 to 23, 25 to 27, 29, 31 to 38), the zirconia sintered body is excellent. It is recognized that it has fracture toughness, exhibits excellent translucency, and is also excellent in water heat deterioration resistance. On the other hand, in the case of a zirconia sintered body having a stabilizer (yttrium oxide and / or ytterbium oxide) content of less than 3.5 mol%, the addition of niobium oxide and / or tantalum oxide can improve the fracture toughness value. Although it is recognized, it is inferior in translucency and is not suitable as a dental restoration material (Sample Nos.
  • the zirconia sintered body having a stabilizer (yttrium oxide and / or ytterbium oxide) content of more than 5.0 mol% has a low fracture toughness value even when niobium oxide is added, and is inferior in mechanical properties. It is not suitable as a dental restoration material (Sample Nos. 39 to 44).

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Cited By (1)

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Publication number Priority date Publication date Assignee Title
WO2024029228A1 (ja) * 2022-08-04 2024-02-08 共立マテリアル株式会社 ジルコニア焼結体

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WO2009001739A1 (ja) * 2007-06-22 2008-12-31 Murata Manufacturing Co., Ltd. 高温構造材料と固体電解質形燃料電池用セパレータ
JP2010514665A (ja) * 2006-12-29 2010-05-06 スリーエム イノベイティブ プロパティズ カンパニー ジルコニア体及び方法
JP2015127294A (ja) * 2013-12-27 2015-07-09 アキュセラ インコーポレイテッド 加工性ジルコニア及び加工性ジルコニアの製造方法

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US20230052915A1 (en) 2019-12-26 2023-02-16 Kuraray Noritake Dental Inc. Production method for machinable zirconia composite sintered body, raw material composition for machinable zirconia composite sintered body, and machinable zirconia composite pre-sintered body

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